CN105862007A - Method for generating Cu triangular crystals in Cu thin film system - Google Patents
Method for generating Cu triangular crystals in Cu thin film system Download PDFInfo
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- CN105862007A CN105862007A CN201610225663.2A CN201610225663A CN105862007A CN 105862007 A CN105862007 A CN 105862007A CN 201610225663 A CN201610225663 A CN 201610225663A CN 105862007 A CN105862007 A CN 105862007A
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- thin film
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
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- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Physical Vapour Deposition (AREA)
- Photovoltaic Devices (AREA)
Abstract
The method discloses a method for generating Cu triangular crystals in a Cu thin film system. The method for generating the Cu triangular crystals in the Cu thin film system comprises the following steps: depositing a Cu thin film on a substrate with <111> crystal orientation; then depositing a layer of thin film which has relatively high reducibility and is made of other materials on the Cu thin film so as to prevent the Cu thin film from being oxidized at high temperature; annealing a sample in an inert gas atmosphere by using heat treatment equipment, wherein the annealing temperature is greater than 500 DEG C; and after insulating for a certain time, cooling in a furnace to obtain the Cu triangular crystals. The surfaces of the obtained Cu triangular crystals are in the shape of an equilateral triangle.
Description
Technical field
The invention belongs to technical field of nano material, relate to the preparation of nano material, be specifically related to Cu thin film
System generates the preparation method of Cu triangle crystal.
Background technology
Along with the development of nanometer technique, the light being different from block materials that micro Nano material is had due to it,
The performances such as electricity, magnetic, have broad application prospects in fields such as catalysis, photoelectricity, microelectronics.Due to micro-nano
The physical and chemical performance of material is strongly dependent on its size or pattern, and its pattern and size Control are always green wood
Technological difficulties in material field.At present, people have developed multiple method, such as hydro-thermal method, electrochemical deposition
Method, metallo-organic compound thermal decomposition method, microemulsion method etc., be successfully prepared the micro Nano material of different-shape,
Such as cube, spherical, star, rod, cage type, dendriform, snowflake shape etc..
Cu nano material is as important raw material, because of the advantage that its should cost having is low, microelectronics,
The fields such as photoelectric functional material, advanced lubrication oil additive, electrocondution slurry, antibiotic bactericide are obtained for extensively
Application.In recent years, research worker uses different methods to be prepared for different Cu nano materials, as copper is micro-
Popped rice, copper dendrite, copper nano-wire etc., but, for using annealing way, it is tied to form product at Cu thin-film body
The method of raw Cu triangle crystal, have not been reported now.
Summary of the invention
The invention provides a kind of method generating Cu triangle crystal under annealing conditions in Cu thin film system.
For reaching above-mentioned purpose, present invention employs techniques below scheme:
Prepare Cu thin film system: in the substrate with<111>crystal orientation, be sequentially depositing Cu thin film and have stronger
Reproducibility and with Cu occur chemical reaction material film, prepare Cu thin film system；
Annealing: use Equipment for Heating Processing in atmosphere of inert gases, Cu thin film system to be annealed, annealing temperature
Degree is more than 500 DEG C, and the upper limit of annealing temperature is as the criterion not melting sample, cools to room temperature after annealing with the furnace,
To Cu triangle crystal；
The temperature retention time of described annealing is not less than 2 minutes.
Have relatively strong reducing property and not with Cu occur chemical reaction material be Mg, Al, Zn, Fe, Sn or
Ti。
Beneficial effects of the present invention is embodied in:
The present invention first successive sedimentation Cu film and there is relatively strong reducing property in the substrate with<111>crystal orientation
The thin film of other materials obtains Cu thin film system, then anneals Cu thin film system, finally thin at Cu
Film system generates Cu triangle crystal.Obtained Cu triangle plane of crystal, becomes positive equilateral triangle.
The method, provides thinking for preparation Cu nanocrystal.
Accompanying drawing explanation
Fig. 1 is the scanning electricity of a certain Cu triangle crystal generated after Ti/Cu/Si (111) thin film system 700 DEG C is annealed
Sub-microscope (SEM) figure, its length of side is about 7 μm.
Fig. 2 is the SEM of a certain Cu triangle crystal generated after Ti/Cu/Si (111) thin film system 700 DEG C is annealed
Figure, its length of side is about 6 μm.
Detailed description of the invention
The invention will be further described with embodiment below in conjunction with the accompanying drawings.
Embodiment
A kind of Ti/Cu/Si (111) thin film system generates the preparation technology of Cu triangle crystal, specifically comprises the following steps that
Wafer Cleaning: use single-sided polishing (111) silicon chip as substrate, before sputtering, use acetone, nothing respectively
Water-ethanol, deionized water ultrasonic cleaning 15 minutes, then dry half an hour.
Sputtering: it is thin that Ti/Cu prepared by Explorer 14 sputter using Denton Vacuum company of the U.S. to produce
Film；Cu target and Ti target being separately mounted on two d.c. sputtering target rifles, the purity of two targets is
99.999%.Before Jian She, the silicon chip cleaned up is put into sputtering chamber, be evacuated to 2 × 10-5Pa.Cu and Ti
Sputtering power be respectively 99w and 105W, sputter rate is respectively 0.4nm/s and 0.12nm/s.The company of employing
Continuous sputtering mode, by controlling sputtering time, preparation 20nmTi/70nmCu/Si<111>thin film (sample).
Annealing: use Equipment for Heating Processing, in argon atmosphere, sample is carried out short annealing.Annealing temperature is
700 DEG C, the annealing heating-up time is 100s, and temperature retention time is 30 minutes, then furnace cooling.
The upper limit of annealing temperature is as the criterion not melting sample.When annealing temperature is less than 500 DEG C, Cu will not be produced
Triangle crystal, annealing time is too short, also will not produce Cu triangle crystal.
The Main Function of the Ti film on thin film system top layer: protection Cu film, prevents it the most oxidized.
The Cu triangle crystal that the present embodiment prepares in Cu thin film system sees Fig. 1 and Fig. 2, obtained
Cu triangle plane of crystal, become positive equilateral triangle.
The above, only a kind of detailed description of the invention of the present invention, but protection scope of the present invention is not limited to
In this, any those familiar with the art is in presently disclosed technical scope, according to this
Bright technical scheme and inventive concept equivalent or change in addition thereof, all should contain in protection scope of the present invention
Within.
Claims (2)
1. the method generating Cu triangle crystal in Cu thin film system, it is characterised in that: include following
Step:
Prepare Cu thin film system: in the substrate with<111>crystal orientation, be sequentially depositing Cu thin film and have stronger
Reproducibility and with Cu occur chemical reaction material film, prepare Cu thin film system；
Annealing: use Equipment for Heating Processing in atmosphere of inert gases, Cu thin film system to be annealed, annealing temperature
Degree is more than 500 DEG C, and the upper limit of annealing temperature is as the criterion not melting sample, cools to room temperature after annealing with the furnace,
To Cu triangle crystal；
The temperature retention time of described annealing is not less than 2 minutes.
The method generating Cu triangle crystal in Cu thin film system the most according to claim 1, it is special
Levy and be, have relatively strong reducing property and not with Cu occur chemical reaction material be Mg, Al, Zn, Fe,
Sn or Ti.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610225663.2A CN105862007B (en) | 2016-04-12 | 2016-04-12 | A method of generating Cu triangle crystal in Cu thin film systems |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610225663.2A CN105862007B (en) | 2016-04-12 | 2016-04-12 | A method of generating Cu triangle crystal in Cu thin film systems |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105862007A true CN105862007A (en) | 2016-08-17 |
| CN105862007B CN105862007B (en) | 2018-08-10 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610225663.2A Active CN105862007B (en) | 2016-04-12 | 2016-04-12 | A method of generating Cu triangle crystal in Cu thin film systems |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101122006A (en) * | 2006-08-10 | 2008-02-13 | 中国科学院微电子研究所 | Preparation method of metal nanocrystalline film |
| US20110065236A1 (en) * | 2009-09-17 | 2011-03-17 | National Taiwan University | Method for maintaining a smooth surface of crystallizable material |
| CN102994953A (en) * | 2012-12-03 | 2013-03-27 | 西安交通大学 | Method for generating dendritic crystal pattern on surface of Cu/Ti film |
-
2016
- 2016-04-12 CN CN201610225663.2A patent/CN105862007B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101122006A (en) * | 2006-08-10 | 2008-02-13 | 中国科学院微电子研究所 | Preparation method of metal nanocrystalline film |
| US20110065236A1 (en) * | 2009-09-17 | 2011-03-17 | National Taiwan University | Method for maintaining a smooth surface of crystallizable material |
| CN102994953A (en) * | 2012-12-03 | 2013-03-27 | 西安交通大学 | Method for generating dendritic crystal pattern on surface of Cu/Ti film |
Non-Patent Citations (1)
| Title |
|---|
| 郭菲等: "退火温度对铜薄膜微观结构和织构的影响规律研究", 《中国体视学与图像分析》 * |
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| CN105862007B (en) | 2018-08-10 |
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Effective date of registration: 20211228 Address after: Room 1019-2, science and technology building, 28 Zhujiang Road, Yantai Economic and Technological Development Zone, Shandong Province 264006 Patentee after: Mingshi innovation (Yantai) micro nano Sensor Technology Research Institute Co.,Ltd. Address before: Beilin District Xianning West Road 710049, Shaanxi city of Xi'an province No. 28 Patentee before: XI'AN JIAOTONG University |